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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Single particle trace element analysis of uranium oxide standards with laser-induced breakdown spectroscopy

Femtosecond Laser-Induced Breakdown Spectroscopy (LIBS) was used to analyze over 1000 individual particles of uranium oxide trace element standard CRM124. Intra-granular analysis showed elemental concentrations were consistent across different surface locations on each uranium grain. However, inter-granular comparison revealed large heterogeneity between different grains of the same sample. By comparing the distribution of elemental concentrations across the particle populations, we were able to correctly identify a manufacturing process involving wet chemistry, rather than a dry mixing of two powders to give an overall chemical average. In conclusion, this demonstrates the utility of LIBS as a large-scale single particle analysis tool for nuclear forensics.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Morphological and chemical characteristics of oxide scales formed on δ-Phase plutonium metal alloys I: 3.5 at% ga

Focused ion-beam scanning electron microscopy (FIB-SEM) and three-dimensional (3D) microscopy were applied to characterize the subsurface morphological features of oxide scales formed on an ~3.5 at.% Ga plutonium (Pu) metal alloy. Using the FIB-SEM technique, a number of morphological features formed in the interior of the oxide scale from Pu metal's environmental exposure were observed and identified. Here, Auger electron spectroscopy (AES) was utilized to characterize the cross-sectional composition and chemistry of the oxide scale. The oxide scale formed during inert storage and operational environments has a characteristic internal scale structure that includes a relatively dense oxide layer with some lateral and transverse cracking. Generally, after subsequent exposure to dry air environment, the oxide scale retained most of the original structural and chemical characteristics. However, after aging in a moist air environment, while the oxide scale was found to maintain the chemical characteristics of the source oxide, the scale was found to be on average thinner and without the previously observed internal microcracking, likely the result of spallation of the source scale during exposure to the new environment.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Morphological and chemical characteristics of oxide scales formed on δ-phase plutonium metal alloys II: 2.0 at% Ga

The focused ion-beam scanning electron microscopy (FIB-SEM) and three-dimensional (3D) microscopy were applied to characterize the subsurface morphological features of oxide scales formed on an ~2.0 at. % Ga plutonium (Pu) metal alloy. Using the FIB-SEM technique, a number of morphological features formed in the interior of the oxide scale from Pu metal’s environmental exposure were observed and identified. Auger electron spectroscopy (AES) was utilized to characterize the cross-sectional composition and chemistry of the oxide scale. The oxide scale formed during inert storage and operational environments was found to be highly variable in thickness and morphology, presenting some regions with a thin (<400 nm), dense oxide layer and others with a thick (>2 µm) scale with substantial lateral cracking. After subsequent exposure to dry air environment, the oxide scale became thicker (~4 µm) and slightly more porous. The changes following aging in a moist air environment were observed to be more severe, with the formation of a highly porous internal structure containing significant lateral and transverse cracking. In comparison to the scale formed on an ~3.5 at. % Ga-Pu metal alloy, the oxide morphology of the lower gallium alloy investigated here exhibited greater variation in thickness and a noteworthy dependence on the presence of water vapor, particularly in terms of the internal porosity formed during growth of the oxide.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Resolving Mixtures of Soot Characterized by SP-AMS Spectra Using a Latent Dirichlet Allocation Model

Soot produced by detonation or combustion events exhibits different chemical properties depending on the fuel, device construction, and environmental conditions in which the event occurs. These properties can be useful for defining relevant signatures for probabilistically identifying the different types of events that occurred, based on the soot that is produced from these events. However, it is rare to observe samples of soot from a detonation or combustion that are not contaminated by outside particles. In this paper, we present a method for resolving mixtures of soot to determine the contributions of sources that may be present in samples of recovered soot. We use Latent Dirichlet Allocation to describe the generative process for a sample of recovered soot, and use Variational Bayesian Inference to learn about the parameters associated with the generative model. We demonstrate the utility of this method by considering real samples of mixtures of soot under various frameworks to show that the model is able to identify the different components present in a sample of soot as well as their mixing proportions.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Ambient Mass Spectrometry Rapid Analysis Methods for Trace Inorganics

The ability to rapidly detect and characterize the chemistry of trace quantities of inorganic species has multiple potential applications, including nuclear safeguards, nuclear forensics, and environmental monitoring. Some mass spectrometric methods currently exist, but they are costly and time-intensive, often destroying chemical information in the process of ionization. Ambient mass spectrometry is a relatively new analytical method in which samples are introduced to the mass spectrometer from atmospheric pressure, rather than from high vacuum. Ambient MS can operate with gentler ionization methods such as electrospray ionization (ESI) and paper-spray ionization (PSI), reducing fragmentation and preserving the chemical information of the analyte. This may be useful for determining the intended purpose of material in a sample. Strontium, part of nuclear fallout, is analyzed here to test these new analytical methods for viability. Electrospray ionization mass spectrometry functions by spraying the sample as a solution through a needle charged to a few kV. A nebulizing gas flows out along with the sample to create the spray before droplets enter a drying chamber with heated drying gas to remove the solvent molecules. From there bare analyte ions enter the mass spectrometer. This method has the advantage of relatively fast sample preparation and stable ionization. More stable ionization produces higher-quality data. Paper-spray ionization mass spectrometry operates by applying sample to a paper triangle. The paper triangle is then electrified in a metal clamp to a few kV before spray solvent is applied. The spray solvent transports analyte in the sample to the tip, where it is ionized and enters the mass spectrometer. One advantage of this method is reduced sample preparation - an analyst can even swipe a surface and cut a triangle directly from the swipe. The data analysis serves to rapidly process tens of samples all at once. The mass spectrometer outputs a file containing a few hundred spectra for each sample. The pipeline processes each one to identify peaks of interest. A full palette of data analysis metrics are generated, including plots of the raw data and plots of calculated values such as isotopic ratios. The pipeline filters the raw data to remove noise and background peaks, as well as peaks representing detector saturation. A heat map is generated to show the overall spectrum in mass-time- intensity space. Post-processing, we obtained the desired calibration curves, demonstrating that both ESI-MS and PSI-MS are viable methods for quantifying trace amounts of inorganics while retaining their chemical speciation information. ESI-MS demonstrated a linear response region of 100 ppb to 20 ppm, with a limit-of-detection of around 100 ppb. At top left is an example spectrum with the {sup 88}SrNO{sub 3} peak identified to show the retention of chemical speciation. PSI-MS showed a linear response region of around 1 ppb to 1 ppm, with a limit-of-detection of near 1 ppb. PSI-MS produced more erratic results than ESI-MS, likely due to the variability in ionization resulting from manual positioning of the paper triangle near the MS inlet. Future efforts will focus on improving the repeatability of PSI-MS as well as analyzing other species of interest such as cerium and uranium. Improvements will also be made to create more reliable data extraction and intelligent data filtering.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2026

Radioisotope dating of nuclear materials using cryogenic decay energy spectrometry

Cryogenic decay energy spectrometry provides high energy resolution and enables absolute decay counting, offering an alternative measurement technique for radiochronometry. A cryogenic decay energy spectrometry experiment was conducted using a magnetic microcalorimeter to determine the age of a plutonium sample. The energy resolution was measured at 0.05% from 5 to 6 MeV. The time since sample purification was determined using the measured concentration ratio of the 241 Am/ 241 Pu radiochronometer. Sample age estimates based on 241 Pu alpha-decay and beta-decay counts, along with 241 Am decay counts, align with the expected sample age within expanded uncertainty (k = 2), supporting the accuracy of cryogenic decay energy spectrometry as a radiochronometric method.

and nuclear chemistry↗
DOE OSTI2023

Routine Beryllium-10 analysis from post-detonation debris and geologic materials [Slides]

Beryllium (Be) isotope measurements provide insight into weapon design, yield, etc. Sample preparation nor measurement capability currently existed at LANL. Potential capability directly benefits nuclear forensics venture. PI Goehring has nearly 20 years of Be chemistry experience, including method implementation with difficult samples.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2021

Materials and Fuels Complex Five-Year Mission Strategy (FY21- FY25)

The Idaho National Laboratory (INL), through its designated mission of advancing innovative nuclear energy solutions, is actively engaged in the research, development, demonstration and deployment of advanced nuclear technology, as well as in fostering private-public partnership for technology development. Key to the success of INL’s mission is the Materials and Fuels Complex (MFC), the only complex in the U.S. that hosts a world-class assemblage of facilities, capabilities and instruments for handling, testing, and characterizing radioactive materials. Driven by its mission/vision of “Engineering and Experiments that Drive the World’s Nuclear Energy Future,” MFC is at the center of INL’s – and indeed the Department of Energy’s – advanced nuclear technology development initiatives, providing essential capabilities such as engineering-scale high-assay low-enriched uranium (HALEU) fuel production, reactor demonstration facilities, post-irradiation examination, and transient irradiation testing. Furthermore, MFC provides an ideal environment for test beds that are utilized for research, development and demonstration (RD&D) activities on used fuel treatment, nuclear non-proliferation, forensics, and nuclear power sources used for space exploration missions conducted by the National Aeronautics and Space Administration (NASA).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

In-situ Synthesis of PuCl 3 and Corresponding Raman and Density Functional Theory Vibrational Modes

The experimental and calculated Raman spectrum of PuCl 3 has been reported for the first time. PuCl 3 is a primary species found in plutonium metal refinement, specifically in pyrochemical salt processes including multicycle direct oxide reduction, metal chlorination, and electrorefining. As such, Raman signatures of PuCl 3 could serve as potential forensic indicators of material process history. A novel technique for synthesizing PuCl 3 from the in situ chlorination of plutonium metal with HCl was developed to establish these signatures. Cerium metal surrogates were utilized to ensure optimization of the plutonium experiments and to minimize personnel exposure, and all experiments were carried out in a Raman reaction chamber designed for air-tight, high vacuum environments. In situ Raman spectroscopy was employed in conjunction with density functional theory (DFT) to investigate the vibrational modes of PuCl 3 . Associated mixed oxy and hydroxyl phases are also reported. The combined Raman and DFT results have eliminated inconsistencies in Raman mode assignments for the MX 3 family of metal chlorides having P6 3 /m symmetry, and IR modes derived from the DFT calculations are additionally presented. The data observed in this study are of potential interest to nuclear forensic analyses, nuclear sample aging, nuclear energy, plutonium processing, and stockpile stewardship.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In-situ Synthesis of PuCl 3 and Corresponding Raman and Density Functional Theory Vibrational Modes

The experimental and calculated Raman spectrum of PuCl 3 has been reported for the first time. PuCl 3 is a primary species found in plutonium metal refinement, specifically in pyrochemical salt processes including multicycle direct oxide reduction, metal chlorination, and electrorefining. As such, Raman signatures of PuCl 3 could serve as potential forensic indicators of material process history. A novel technique for synthesizing PuCl 3 from the in-situ chlorination of plutonium metal with HCl was developed to establish these signatures. Cerium metal surrogates were utilized to ensure optimization of the plutonium experiments and to minimize personnel exposure, and all experiments were carried out in a Raman reaction chamber designed for air-tight, high vacuum environments. In-situ Raman spectroscopy was employed in conjunction with Density Functional Theory (DFT) to investigate the vibrational modes of PuCl 3 . Associated mixed oxy and hydroxyl phases are also reported. The combined Raman and DFT results have eliminated inconsistencies in Raman mode assignments for the MX 3 family of metal chlorides having P6 3 /m symmetry, and IR modes derived from the DFT calculations are additionally presented. The data observed in this study is of potential interest to nuclear forensic analyses, nuclear sample aging, nuclear energy, plutonium processing, and stockpile stewardship.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Machine learning in analytical spectroscopy for nuclear diagnostics [Invited]

Analytical spectroscopy methods have shown many possible uses for nuclear material diagnostics and measurements in recent studies. In particular, the application potential for various atomic spectroscopy techniques is uniquely diverse and generates interest across a wide range of nuclear science areas. Over the last decade, techniques such as laser-induced breakdown spectroscopy, Raman spectroscopy, and x-ray fluorescence spectroscopy have yielded considerable improvements in the diagnostic analysis of nuclear materials, especially with machine learning implementations. These techniques have been applied for analytical solutions to problems concerning nuclear forensics, nuclear fuel manufacturing, nuclear fuel quality control, and general diagnostic analysis of nuclear materials. The data yielded from atomic spectroscopy methods provide innovative solutions to problems surrounding the characterization of nuclear materials, particularly for compounds with complex chemistry. Implementing these optical spectroscopy techniques can provide comprehensive new insights into the chemical analysis of nuclear materials. In particular, recent advances coupling machine learning methods to the processing of atomic emission spectra have yielded novel, robust solutions for nuclear material characterization. This review paper will provide a summation of several of these recent advances and will discuss key experimental studies that have advanced the use of analytical atomic spectroscopy techniques as active tools for nuclear diagnostic measurements.

Rao, Ashwin P. (ORCID:0000000319312568)↗